CN103623822B - Take magnesia as the method that rich copper type magnesium copper composite oxide of metal prepared by raw material - Google Patents
Take magnesia as the method that rich copper type magnesium copper composite oxide of metal prepared by raw material Download PDFInfo
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- CN103623822B CN103623822B CN201310638971.4A CN201310638971A CN103623822B CN 103623822 B CN103623822 B CN 103623822B CN 201310638971 A CN201310638971 A CN 201310638971A CN 103623822 B CN103623822 B CN 103623822B
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Abstract
Take magnesia as the method that rich copper type magnesium copper composite oxide of metal prepared by raw material, relate to the method preparing magnesium copper composite oxide of metal, the first step, with activated magnesia and copper chloride for raw material, prepare rich copper type magnesium copper composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; 3rd step, is made into the aqueous solution by copper chloride, is added drop-wise in hydrated magnesium complex solution.4th step, obtains CuO-Cu4MgO5 magnesium copper composite metal oxide by emulsion suction filtration, washing, dry rear calcining.Utilize activated magnesia and copper chloride to prepare rich copper type magnesium copper composite oxide of metal for raw material, make use of metal ion match copolymerization phenomenon in the aqueous solution, form metal ion water and hydroxyl copolymer, without any additive, method is simple.The CuO-Cu4MgO5 magnesium copper composite metal oxide prepared has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
Description
Technical field
The present invention relates to a kind of method preparing composite oxide of metal, particularly relating to magnesia is the method that rich copper type magnesium copper composite oxide of metal prepared by raw material.
Background technology
China is magnesium resource big country, and magnesite gross reserves is 3,100,000,000 tons, accounts for more than 1/4th of world's gross reserves, and high value added utilization magnesite becomes the emphasis of research.
Because cupric oxide and magnesia can be used as catalyst in a lot of reaction, and composite metal oxide has the many character being better than single metal oxide, with MgO and CuCl2 for raw material reaction obtains presoma magnesium copper composite metal hydroxide, obtaining after calcining is the CuO-Cu4MgO5 catalyst of Cu4MgO5 through XRD analysis molecular formula, the magnesium copper composite metal oxide of preparation is the composite oxides with bimetallic center, can be used as catalyst or the carrier of some organic reflection, wherein Mg can suppress the carrying out of side reaction in chemical reaction as alkali center.Cu in Cu4MgO5 catalyst and the Cu in Supported CuO, as acid centre, can obtain because it has non-shared electron the carrying out that organic electronics promotes organic reaction.
The composite metal oxide that magnesium is relevant with copper all has good application background at catalytic field, as Al-Mg composite metal oxide, magnesium manganese composite metal oxide, magnesium iron composite metal oxide, copper cobalt composite metal oxide, copper-chromic composite metal oxide, copper iron composite metal oxide etc.Wherein most composite metal oxide has good application in solid propellant.As magnesium iron composite metal oxide, copper cobalt composite metal oxide, copper-chromic composite metal oxide, copper iron composite metal oxide to be used in solid propellant as burningrate catalyst time, obviously can reduce the pyrolysis temperature of AP, improve boron powder once with second-time burning efficiency, after carrying out further modification, coated process to catalyst, catalytic performance is got back and is further improved, and have also been obtained solution with the compatibility of end hydroxy butadiene in system.In magnesium copper composite metal oxide, the interaction of Cu and Mg is conducive to the activation of active sites, thus can improve the reaction condition such as catalytic performance, reduction reaction temperature.Cupric oxide is a kind of common catalyst or catalyst carrier, in a lot of reaction, all demonstrate good catalytic performance.MgO activity position can suppress the carrying out of side reaction in reaction in the reaction.
Spatial network shape metal hydroxy polymer is formed according to the polymerism of bimetallic ion in the aqueous solution.The method is simple to operate, compared with additive method, remains initial native structure; Not high to equipment, technical requirement; Do not introduce other auxiliary agents, product purity is high; Cost is low; Because the OH – in solution discharges gradually, the therefore morphology controllable of products therefrom.
Summary of the invention
The object of the present invention is to provide a kind of method taking magnesia as raw material and prepare rich copper type magnesium copper composite oxide of metal, activated magnesia is dissolved in the water by the method, form aqua oxidation magnesium complex, make use of metal ion match phenomenon in the aqueous solution, without any additive, method is simple, and the CuO-Cu4MgO5 magnesium copper composite metal oxide prepared has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
The object of the invention is to be achieved through the following technical solutions:
Take magnesia as the method that rich copper type magnesium copper composite oxide of metal prepared by raw material, described method with activated magnesia and copper chloride for raw material, prepare rich copper type magnesium copper composite oxide of metal, the method utilizes the copolymerization phenomenon of metal ion match in the aqueous solution, additive-free preparation; The CuO-Cu4MgO5 magnesium copper composite metal oxide prepared has bimetallic center, as catalyst or the carrier of organic reaction; Concrete preparation process comprises: the first step, with activated magnesia and copper chloride for raw material, prepares rich copper type magnesium copper composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; 3rd step, is made into the certain density aqueous solution by copper chloride, is added drop-wise in hydrated magnesium complex solution, the 4th step, and emulsion suction filtration, washing, dry rear calcining are obtained CuO-Cu4MgO5 magnesium copper composite metal oxide.
Advantage of the present invention and effect are:
1. the present invention propose a kind of with activated magnesia and copper chloride for raw material, utilize the polymerism of metal ion in the aqueous solution to prepare rich copper type magnesium copper composite oxide of metal, without any additive, method is simple, and cost is low.
2. prepare CuO-Cu4MgO5 magnesium copper composite metal oxide.
3. the CuO-Cu prepared
4mgO
5magnesium copper composite metal oxide has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
Accompanying drawing explanation
Fig. 1 is present invention process schematic diagram;
Fig. 2 is that product XRD of the present invention schemes;
Fig. 3 is the peak area curve map of the magnesium copper composite metal oxide adsorbent CO2 that differential responses thing proportioning of the present invention obtains;
Fig. 4 is the peak area curve map of the magnesium copper composite metal oxide adsorbent NH3 that differential responses thing proportioning obtains.
Note: Fig. 2-Fig. 4 of the present invention is analysis schematic diagram or the photo (only for reference) of product state, word or the unintelligible understanding do not affected technical solution of the present invention of image in figure.
Detailed description of the invention
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
General principle of the present invention:
The water-soluble generation hydrated magnesium of magnesia, generates hydroxyl magnesium ion then, the aobvious alkalescence of solution, under more polyhydroxyl ion existence condition, forms hydroxyl Hydrated Magnesium Ion complex.
MgO+H
2O→[Mg(OH)] ①
[Mg(OH)]
++ OH
–→[Mg(OH)
2]（aq） ②
[Mg(OH)
2]（aq）+OH
–→[Mg(OH)
3]
–③
[Mg(OH)
3]
–+OH
–→[Mg(OH)
4]
2–④
[Mg(OH)
4]
2–+OH
–→[Mg(OH)
5]
3–⑤
[Mg(OH)
5]
3–+OH
–→[Mg(OH)
6]
4–⑥
And in copper chloride solution, along with copper chloride concentration increases, solution acidic increases, under reaching certain pH value condition, form hydroxyl hydration copper ion complex,
Cu2++ 4H2O→[Cu(H2O)4]2+ ⑦
Cu2++ 4OH–→[Cu(OH)4]2- ⑧
The Acidity of Aikalinity of both utilizations is different, under certain proportion condition, when solution pH value is certain, forms magnesium copper water and the hydroxyl polymeric body of spacial framework.
Basic scheme of the present invention:
The first step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; With second step, copper chloride is made into the certain density aqueous solution, is added drop-wise in hydrated magnesium complex solution.3rd step, obtains CuO-Cu4MgO5 magnesium copper composite metal oxide by emulsion suction filtration, washing, dry rear calcining.
Technical method of the present invention:
This project for raw material with activated magnesia and copper chloride, utilizes the polymerism of metal ion in the aqueous solution, prepares the emulsion of magnesium copper combined polymerization, and after filtration washing drying, calcining obtains CuO-Cu4MgO5 magnesium copper composite metal oxide.
Embodiment 1:
(1) activated magnesia pretreatment, puts into Muffle furnace and calcines 2h at 600 DEG C.After each activity recovery, can use 4 days, re-using after 4 days need first with above-mentioned steps activity recovery again.
(2) taking the activated magnesia 4g after calcining adds in 250ml there-necked flask, adds 100ml distilled water in there-necked flask, 50 DEG C of ultrasonic reaction 1h.
(3) measure 1mol/L copper chloride solution, dropwise add in magnesium oxide solution, drip and terminate its pH value of rear survey, after pH value is stable (about 1.5h), stop experiment.
(4) suction filtration, dry, calcine under 800 DEG C of conditions, 2h, obtain product.
From Fig. 3, Fig. 4, CuO-Cu
4mgO
5magnesium copper composite metal oxide has bimetallic center.
Claims (1)
1. be the method that rich copper type magnesium copper composite oxide of metal prepared by raw material with magnesia, it is characterized in that, described method with activated magnesia and copper chloride for raw material, prepare rich copper type magnesium copper composite oxide of metal, the method utilizes the copolymerization phenomenon of metal ion match in the aqueous solution, additive-free preparation; The CuO-Cu prepared
4mgO
5magnesium copper composite metal oxide has bimetallic center, as catalyst or the carrier of organic reaction; Concrete preparation process comprises: the first step, is dissolved in the water by activated magnesia, forms aqua oxidation magnesium complex; Second step, is made into the aqueous solution by copper chloride, is added drop-wise in hydrated magnesium complex solution, the 3rd step, and emulsion suction filtration, washing, dry rear calcining are obtained CuO-Cu
4mgO
5magnesium copper composite metal oxide;
Concrete preparation process comprises:
(1) activated magnesia pretreatment, puts into Muffle furnace and calcines 2h at 600 DEG C, after each activity recovery, can use 4 days, and re-using after 4 days need first with above-mentioned steps activity recovery again;
(2) taking the activated magnesia 4g after calcining adds in 250ml there-necked flask, adds 100ml distilled water in there-necked flask, 50 DEG C of ultrasonic reaction 1h;
(3) measure 1mol/L copper chloride solution, dropwise add in magnesium oxide solution, drip and terminate its pH value of rear survey, after pH value is stable, stop experiment;
(4) suction filtration, dry, under 800 DEG C of conditions, calcine 2h, obtain product.
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|---|---|---|---|
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|---|---|---|---|
| CN201310638971.4A CN103623822B (en) | 2013-12-04 | 2013-12-04 | Take magnesia as the method that rich copper type magnesium copper composite oxide of metal prepared by raw material |
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|---|---|
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| CN103623822B true CN103623822B (en) | 2015-08-26 |
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|---|---|---|---|---|
| CN103657650A (en) * | 2013-12-10 | 2014-03-26 | 沈阳化工大学 | Preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as raw material |
| CN105413692A (en) * | 2016-01-08 | 2016-03-23 | 沈阳化工大学 | Method for preparing magnesium cobalt metal compound oxide with active magnesium oxide as raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441381A (en) * | 2011-10-28 | 2012-05-09 | 昆山德泰新材料科技有限公司 | Catalyst produced by using copper oxide powder and production method thereof |
| CN103073063A (en) * | 2012-12-17 | 2013-05-01 | 沈阳化工大学 | Method for preparing nanometer magnesium ferrite through utilizing active magnesium oxide as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441381A (en) * | 2011-10-28 | 2012-05-09 | 昆山德泰新材料科技有限公司 | Catalyst produced by using copper oxide powder and production method thereof |
| CN103073063A (en) * | 2012-12-17 | 2013-05-01 | 沈阳化工大学 | Method for preparing nanometer magnesium ferrite through utilizing active magnesium oxide as raw material |
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